8 Formulation & Evaluation of Cosmetics

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Formulation & Evaluation of Cosmetics :

Formulation & Evaluation of Cosmetics




INTRODUCTION The word cosmetic derives from the Greek Kosm tikos meaning 'having the power, arrange, skilled in decorating’. The origin of cosmetics are associated with fighting, hunting, religion and superstition. In 3000 BC, early men used cave painting to attract animals for hunting. Then they became associated with medicine, and later, as knowledge increased, becoming dissociated from medicine. Now, cosmetics is a distinct branch of science with the technologies of its own. 3


SKIN CARE PRODUCTS Cleansing products Skin toners Post-cleansing products Sun protecting agents moisturizers 4

1. Cleansing products:

1. Cleansing products 1.1 SOAP AND SYNTHETIC DETERGENT BASED PRODUCTS Surfactant based soap bars are very effective cleansing agents and were popularly used in the past; but they have some disadvantages which limits their use in modern formulations. The washing solution formed is extremely alkaline, and can cause irritation, dryness and scaling. Rinse-off, liquid products are more popularly used. They can be formulated into many forms: gels, liquids, aerosols. Formulation of liquid/ gel facial cleansers: These formlutaions normally contain a mixture of surfactants , a thickener ( NaCl ), a refatting agent , perfume and water . The appearance can be modified by water-soluble dyes . Pearlescent agents (ethylene glycol stearate derivatives) or opacifiers (Titanium dioxide) can also be used. Surfactants of anionic/ amphoteric faminily are mostly used here; for e.g. alkyl betaines , sulfobetaines and N-alkyl-amino propionates ( amphoteric ) and taurates , sulfosuccinates , fatty alcohol ether sulfates (anionic). 5

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1.2 CLEANSERS FOR OILY SKIN Frequent and effective cleansing is recommended for oily skin in order to reduce the amount of sebum left on the skin. Emulsion cleansers are to be avoided since they tend to leave a layer of oil on the skin. Formulation: Synthetic detergent systems can be used for cleansing oily skin where an astringent (ethanol or Pyridoxine tripalmitate ) may be included for use in oily/sensitive skin. 1.3 EMULSION CLEANSERS Cleansing cream- one of the oldest-known emulsions and is commonly known as a cold cream because application to the skin results in a cooling effect which is produced from slow evaporation of the water contained in the emulsion. Rinse-off emulsions- these are applied or massaged into the face and rinsed off with water. They may generate a small amount of lather whilst being washed off and are known as foaming cleansers. 6

Formulae for cleansing creams:

7 Formulae for cleansing creams

2. Skin toners:

2. Skin toners Skin toners are also called as fresheners , clarifying lotions, tonics and astringents . When applied onto the skin, toners remove the final traces of grime, residues from soap or emulsion cleaners plus any loose flakes of dead skin. They leave the skin feeling clean, fresh and used before a moisturizer or liquid foundation make-up is applied. The active component of these products is astringent. Denatured ethanol (5-25%.) is commonly used as the astringent material. Astringent lotions- are useful in the control of very oily or acne-prone skin. These products often contain high levels of ethanol and sometimes isopropanol . Toners and fresheners- Toners for dry and normal skin are often based on lower alcoholic strengths. At the present time alcohol-free toners are often preferred since alcohol can leave the skin dry. 8

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3. Post-cleansing products:

3. Post-cleansing products After cleansing, skin becomes dry. This can be reversed by using some cosmetics i.e. moisturizers. Moisturizing preparations can be classified into five groups. 1. Day preparations. 2. Night preparations. 3. Hand and body lotions. 4. All-purpose products. 5. Barrier creams. 1. Day preparations: these are light, oil-in-water emulsions which are designed to spread easily and rub into the skin quickly. The formulation is based on high-quality stearic acid as the oil phase. 2. Night preparations: these are water-in-oil emulsions which are available as creams and viscous lotions. They are less cosmetically elegant than the oil-in-water types because of the difficulty of rubbing them in. Traditional night creams were originally based on the beeswax, borax and mineral oil systems. Today other waxes, vegetable oils and silicone oils (instead of mineral oil) can be used as emollients and co-emulsifiers. 10

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3. Hand and body lotions Products for use on the hands and body tend to be similar in formulation to the day moisturizers. They generally contain a high level of the humectants. The distilled lanolin alcohols may be added to improve the barrier-forming properties on the skin. 4. All-purpose products They can be used as a moisturizer or a cleansing cream on the face, hands and body. 5. Barrier creams Barrier creams, like hand creams, are protective products. In addition to acting as moisturizers, they prevent external materials from permeating the skin. The formulation of barrier creams will be determined by the type of external materials from which the user requires protection. 11

Special additives/nutrients for skin care products:

Special additives/nutrients for skin care products VITAMINS The most commonly used vitamins include E, A, C and panthenol . Vitamin E (alpha- tocopherol ) is employed as an antioxidant/free radical scavenger. Retinoids ( trans retinoic acid or tretinoin ) have been most widely used in the treatment of photo damaged skin. Vitamin C (ascorbic acid) is another natural antioxidant which regulates collagen biosynthesis and is involved in the wound-healing process of the body. PROTEINS hydrolysed protein, amino acids and proteoglycansare very substantive to the skin, leaving it feeling soft and smooth. Example- collagen, hyaluronic acid, milk proteins, silk proteins and amino acids. ESSENTIAL FATTY ACIDS 7-Linolenic acid (GLA) is an essential fatty acid which occurs naturally in many vegetable seed oils. GLA is said to improve the skin's efficiency as a barrier to transepidermal water loss. Also , α - hydroxy acids , β - hydroxy and α - keto acids are added for use in aging; β - Glucans are added in management of wound-healing. 12

4. Sun Protecting Agents:

4. Sun Protecting Agents UV rays (wavelength 100-400nm) have the highest energy among all of the wavelengths emitted from the sun which reaches to Earth’s surface. Among the sub-regions of UV region, UV-B & UV-A are mostly responsible for the phototoxic reactions in human (sunburn, skin cancer, aging, photodermatosis etc.). So, a sunscreen product must have the following criteria: It must absorb UV light over a broad or specified part of the spectrum without any chemical breakdown, It must be resistant to removal by water or sweat, It must not require too-frequent re-application to be effective. It must be highly effective at low concentrations. It must be non-toxic, non-irritant and non-sensitizing. The level of protection from sunburn afforded by a sun product is described by the sun protection factor (SPF). The SPF is measured in vivo using human volunteers following a strict method.SPF measures sunburn, so it is predominantly a measure of UVB protection. 13


INGRADIENTS Sunscreen agent : p-amino benzoic acid derivatives, cinnamates salicylates camphor derivatives [3-(4-methylbenzylidine)camphor] inorganic sunscreens [talc, mica, ZnO , kaolin] Waterproofing agents: silicone oils [ dimethicone , cyclomethicone ] polymers [ alkylated polyvinylpyrrolidone ] Emollients and diluents: propylene glycol, isopropyl myristate , lanolin, mineral oil, castor oil etc. Humactants : glycerol, sorbitol Thickeners: carbomer Rheology modifier: xanthane gum, Magnesium aluminium silicate 14


FORMULATIONS: Sunscreen products can take a number of forms such as gels, sticks, oils or emulsions. 4.1 GELS These are an extremely attractive and elegant formulation type. Their main drawbacks lie in their potential irritancy where alcohol is part of the formula, and their relatively low SPF and water-resistant properties. 4.2 STICKS These are useful for direct application of sunscreens to a specific small area such as the nose, lips or forehead. They are usually good water-repellents due to the presence of oils and waxes. The choice of waxes determines the melting point of the stick and its performance on the skin. 4.3 OILS They are convenient to use and have a good level of water resistance due to their oily nature. However, only low SPFs can be achieved due to the limitation of sunscreen solubility and the production of a very thin transparent film on the skin. 15

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4.4 EMULSIONS: By far the most popular formulation type for sunscreen products. They are able to achieve the highest SPF of all formulation types because they deposit a uniform non-transparent film on the skin. They also have the ability to penetrate the skin's horny layer to some degree, thus increasing their efficacy and durability. The oil phase can contain: • Oil-soluble sunscreen materials. • Oil-soluble antioxidant vitamins, for example vitamin E. • Water-resistant agents, silicones, polymers. • Emollients, esters or oils such as mineral or vegetable oil. • Primary and secondary oil-soluble emulsifiers. The water phase can contain: • Water-soluble sunscreen agents. • Humectants, glycerol, sorbitol . • Primary and secondary water-soluble emulsifiers. • Neutralizing agents. 16

Formulae: emulsion:

Formulae: emulsion W/O O/W 17




HAIR SHAMPOOS Requirements of a shampoo To remove sebum (the secretion of the sebaceous glands) and atmospheric pollutants from the hair and scalp. To remove the residues of previously applied hair treatments, e.g. polymeric constituents from styling lotions and hair sprays. To deliver an optimum level of foam to satisfy the expectation of the user. To leave the hair in a satisfactory condition after rinsing so that it can be combed easily both in the wet and dry state. To perform as a vehicle for the deposition of beneficial materials onto the hair and scalp. To be non-toxic and non-irritating to the hair and the scalp. To be non-damaging to the tissues of the eye if inadvertently splashed 19

Ingredients :

Ingredients Main detergent Class 1: Anionics Alkyl sulfates, Alkyl ether sulfates, sulfosuccinates Class 2: Nonionics Fatty acid alkanolamides , Fatty amine oxides, Alkylpolyglucosides Class 3: Amphoterics Imidazoline derivatives, Alkylamidobetaines and alkylbetaines Class 4: Cationics ‘not used in shapoos ’ Shampoo additives Thickeners Sodium chloride, polyethylene glycol Pearlizers / opacifiers Glycol distearate Preservatives Isothiazolinones , parabens pH modifiers Citric acid

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21 Functional Additives Silicone additives ( dimethicone copolyols , dimethyl siloxane greatly improve combing and antistatic properties at low concentrations, 0.1-0.5%. Proteins and amino acids protein derivatives can influence the mechanical properties of hair fibre , with beneficial effect. Ceramides Increased protection against UV and visible radiation, reduction of the loss of water- solublepolypeptides Panthenol provitamin of pantothenic acid or vitamin B5 Glutamic acid derivatives these derivatives are a source of hair growth energy and that significant linear growth stimulation can be obtained Zinc pyrithione , Piroctone olamine antidandruff agents

Formulations :

Antidandruff 22 Conditioning shampoo Baby shampoo Formulations


HAIR CONDITIONERS Conditioners applied to the hair after shampooing are designed to confer the following properties on the hair: 1. Smooth, tangle-free wet and dry combing. 2. Reduction of static electricity generated by combing and brushing dry hair, otherwise known as 'flyaway' hair. 3. Improved gloss or lustre . 4. Improved body or volume. 5. Improved texture of chemically or heat damaged hair. Formulation: The cationic wetting agent , cetyl trimethyl ammonium chloride (CTAC) is the key ingredient. The hair has an anionic (- ve ) charge, and anything with a cationic charge (+ ve ) will be attracted to the hair and attach itself to the hair shaft. Hence the friction between hair & comb is reduced, ultimately reducing the ‘flyaway’. 23

Formulae :

Hair conditioner Intensive hair conditioner 24 Formulae




1. ANTIPERSPIRANTS & DEODORANTS An antiperspirant actively reduces the amount of underarm perspiration. Whereas, A deodorant masks and/or reduces axillary odour through the use of an antimicrobial agent or a fragrance. Means, it can be said that “ a 'deodorant' is not an 'antiperspirant‘, but an 'antiperspirant' is automatically a 'deodorant' .” ANTIPERSPIRANT ACTIVE INGREDIENTS: The main ingredient is the water-soluble aluminium complexes ( aluminium dichlorohydrate , aluminium sesquichlorohydrate , aluminium chlorohydrate -ACH). cationic zirconium compounds have shown synergistic effect with ACH Buffering agents ( glycine and urea) can be added alongwith active ingredients. 26

Formulations :

Formulations a) CREAMS Creams are one of the first products. These oil-in-water emulsions required acid-stable emulsifying agents. consumers had to apply them with their fingers to the axillae . b) STICKS and SOLIDS Typically based on sodium stearate as the gelling agent (either propylene glycol or alcohol). They also contain an anti-microbial agent, humectant and perfume. These formulations are aesthetically pleasant and have excellent application characteristics, but the antiperspirant efficiency is low. c) ROLL-ONS One of the most popular carrier forms of antiperspirant. There are several types of roll-ons depending upon their formulation base. For e.g. Water, alcohol, hydro-alcoholic systems, esters and silicones. Water-based roll-on (o/w)- usually an oil-in-water emulsion. They show an excellent physical stability and ease of application. 27


Formulations Alcohol-based and hydro-alcoholic roll-ons- they allow a shorter drying time. Only actives with adequate alcohol solubility works in this system (e.g. alcohol soluble ACH, aluminium zirconium pentachlorohydrate ). Clear water-in-oil roll-ons- These are relatively new on the market. They demonstrate superior aesthetics and leave no residue or deposit on the skin after application. 28 Water-based roll-on Alcohol-based roll-on


Formulations d) AEROSOLS These are the most widely used products till date. The main advantage of this system is it doesn’t not involve the container or the product coming in contact with the skin of the user. Usually in these preparations, enhanced efficiency aluminium chlorohydrate is used as active. A hydrocarbon propellant system is included in the formulation. 29


2. SHAVING PRODUCTS Shaving is now a days a regular practice by men, and it is an important part of grooming as well as a social necessity. MECHANISM : the shaving products allows Wetting of the hair fibre and cause it to swell and soften and to lower the force required to cut the hair, reducing discomfort during shaving. Also, some degree of lubrication of the skin is necessary for a reasonably comfortable shave. There are a number of formulation shaving products available in market now, like- lather shaving creams, sticks, shaving foams, gels, shaving oils and more. 2.1 LATHER SHAVING CREAM They are based on a mixture of sodium and potassium soaps, potassium soaps are more readily soluble than sodium soaps and they help to generate foam more quickly. A properly formulated product should therefore provide a copious lather of small bubbles, which break slowly and remain on the beard throughout the duration of the shave to provide sufficient emolliency . 30

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A lather shaving cream generally contains 30-50% of soaps (usually stearic acid) combined with coconut oil fatty acids. A humactant (glycerol, sorbitol ) is also included in the formulation. 2.2 AEROSOL SHAVING FOAM: The aerosol can is filled with a soap solution (concentrated), together with liquid propellant added under pressure. On shaking, some of the propellant becomes temporarily emulsified in the concentrate. When the valve is actuated the propellant pushes the concentrate out of the valve. On reaching atmospheric pressure the emulsified propellant expands to form an instant foam. They generally contain triehtanolamine as cation , instead of NaOH / KOH. 31


formulae 32


3. AFTER-SHAVE PRODUCTS This products are used to- Alleviate after-shave skin trauma, To cool and refresh skin, Exert mild astringent effect. 3.1 AFTER-SHAVE LOTION Most popular type product, containing about 40-50% of ethanol and the appropriate level of water. The ethanol/water ratio may be adjusted depending on the type and level of perfume. In some instances it is necessary to use a perfume solubilizer . Other ingredients include: propylene glycol as humectants ; menthol as cooling agent ; witch hazel as astringent , quaternary ammonium compounds as biocides , and di -isopropyl adipate as emollient . 33

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3.2 After-shave gel Gels are made by using a combination of a carboxyvinyl polymer (A) and a base (B). The stiffness of the gel can be altered by varying the amount of the polymer and the triethanolamine addition. 34



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For evaluating the efficacy of a cosmetic product it is necessary to carry out studies on ‘human volunteers’. Therefore, a panel of human subjects are formed which must be under the strict supervision of an ethical committee. During study, ethical standards must be carefully observed. Scientific, legal and lay representatives should be included in the ethical committee and their function is to make an independent evaluation of new test protocols. CORE STRUCTURE OF STUDY : Selection of a suitable test panel, Preconditioning period, Baseline assessment, Questionnaire Post-treatment period Product crossover. 36


EVALUATION OF SKIN-CARE PRODUCTS The various methods developed for evaluating skin moisturizing effects include: 1 . STUDY OF SKIN MORPHOLOGY: It involves evaluation of gross or microscopic changes in the physical appearance of the skin. For e.g. while testing the efficacy of a moisturizer, the subjects are given with both control and test products for definite time duration; and the outcomes are assessed by skin photography or Scanning Electron Microscopy (SEM). 2 . EVALUATION OF MECHANICAL PROPERTIES OF SKIN: This method includes Measurement of skin friction : to evaluate the degree of skin smoothness or greasiness of the skin. Measurement of skin elasticity : to evaluate firmness or suppleness of skin. Point indentation : to measure skin softness. 37

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3. STUDY OF ELECTRICAL PROPERTIES OF SKIN Keratin is a weak electrical conductor, especially when dry. When skin is moisturized this conductivity increases, as water molecules are strongly dipolar and combine very readily with the keratin chains. Measurement of skin electrical properties may therefore provide information on the degree of hydration of the skin. 4. TRANSEPIDERMAL WATER LOSS (TEWL) In involves measurements of the rate of evaporative water loss from the skin surface before and after various treatments. 38

Evaluation of sunscreen products:

Evaluation of sunscreen products The efficacy of a sunscreen is measured in terms of sun protecting factor (SPF). SPF value ranges from 2 (minimal) to over 30 ; however above SPF 15 there is more chances of adverse reactions like sensitization. SPF can also be defined in terms of ‘Minimum Erythemal Dose (MED)’ which is the minimum radiation required to produce erythema . SPF testing in-vivo : This is carried out on the skin of the backs of between ten and twenty human volunteers. Initially, the (MED) u is determined by exposing the skin to increasing dose of radiation. The sun product is then applied on a separate area of the back of the subject, and same experiment is repeated to determine (MED) p . Then SPF is calculated using the above formula. 39


EVALUATION OF HAIR-CARE PRODUCTS EVALUATION OF HAIR CONDITIONERS: The resistance to combing is determined by using a comb attached with a spring gauge in-vitro. This method can also be applied in-vivo if needed. Effect on static electricity of dry hair can be measured by using a charge locator, which is actually a valve voltameter in which the grid is connected to a probe. This test also, can be performed both in-vitro and in-vivo. Gloss can be quantified by only in-vitro method. Testing of gloss in-vivo is difficult as it takes into account both reflected and scattered light. EVALUATION OF HAIR SHAMPOOS There are a number of methods to test the efficacy of shampoos according to their purpose and ingredients. The common parameters are- Evaluation of hair greasiness, Evaluation of hair strength and ease of combing, Evaluation of antidandruff formulations. 40

Evaluation of Deodorants:

Evaluation of Deodorants Both in vivo and in vitro methods are available. But In vitro techniques do not provide a reliable indicator of clinical effectiveness. The two principal methods for the in vivo evaluation of deodorant efficacy are- Determination of the effect of treatment on the skin microflora ; Olfactory assessment of the effects on skin odours . In the first method, the axillary skin is tested for quantifying the microflora present in it. In the other method, olfactory assessment of the effect of deodorants on body odours may be performed by direct armpit sniffing or by indirect sniffing of pads. 41

Antiperspirants evaluation:

Antiperspirants evaluation Antiperspirants aim to bring about a temporary decrease in sweat production in the axillae . The most widely used procedure for efficacy testing of antiperspirants is a gravimetric method which involves the collection and weighing of axillary sweat under controlled conditions. The percentage of reduction is calculated according to the following formula: 42

Reference: :

Reference: Mottram F J, Lees C E; Hair Treatments; ‘ Poucher's Perfumes, Cosmetics and Soaps 10 th edition’ ; Springer publication; page: 255-288 Abamba G; Skin Preparartions ; ‘ Poucher's Perfumes, Cosmetics and Soaps 10 th edition’; Springer publication; page: 393-452 Keith Ertel ; Personal Cleansing Products: Properties and Use; ‘Cosmetic Formulation of Skin Care Products ’; page 35-58 Melanie Smith; Toners and Astringents; ‘Cosmetic Formulation of Skin Care Products’; page: 67-75 Roberts M E; efficacy testing of cosmetics and toiletries; ‘ Poucher's Perfumes, Cosmetics and Soaps 10 th edition’ ; Springer publication; page: 555-600 Analysis Of Cosmetic Products; Amparo Salvador & Alvderto C. 43

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